PROCESS FOR THE PRODUCTION OF CARBON BLACK

Abstract

A process for producing surface modified carbon black is disclosed. The process comprises the step of treating carbon black with a sulfur compound in an amount in the range of 0.005%-1% of the carbon black to effect in situ formation of surface groups to produce the surface modified carbon black which when combined with a polymer composition alters the carbon black-polymer interaction to decrease the hysteresis of the polymer composition. The curing time required for polymer composition comprising the surface modified carbon black is also decreased. The preferred sulfur compounds are sulfite or sulfate salts.

Claims

1. A process for producing a surface modified carbon black comprising the step of treating carbon black with a sulfur-containing compound to obtain the surface modified carbon black which when combined with a polymer composition alters the carbon black-polymer interaction to decrease the hysteresis of the polymer composition by at least 1%.

2. The process as claimed in claim 1, wherein the sulfur-containing compound is selected from the group consisting of sodium sulfate, sodium sulfide, sodium sulfite, sodium polysulfide, sodium thiosulfate, phenylene disulfide, alkali metal sulfate, alkali metal sulfite, alkali metal sulfide, alkaline earth metal sulfate, alkaline earth metal sulfite, alkaline earth metal sulfide, and mixtures thereof.

3. The process as claimed in claim 1, wherein the sulfur-containing compound is used in an amount in the range of 0.005-1% of the carbon black.

4. The process as claimed in claim 1, wherein the decrease in the hysteresis of the polymer composition is in the range of 1% to 20%.

5. The process as claimed in claim 1, wherein the sulfur-containing compound is added during the manufacturing of the carbon black.

6. The process as claimed in claim 1, wherein the sulfur-containing compound is added after the manufacturing of the carbon black.

7. The process as claimed in claim 1, wherein the method step of treating carbon black with a sulphur-containing compound is carried out by a technique selected from the group consisting of pouring, spraying, injecting, dispersing and diffusing.

8. The process as claimed in claim 1, wherein the sulfur-containing compound is in the form of dispersion.

9. The process as claimed in claim 1, further comprises a step of mixing the sulfur-containing compound with process water to pelletize the carbon black.

Description

BRIEF DESCRIPTION OF THE ACCOMPANYING DRAWINGS

[0017] The invention will now be described with the help of the accompanying drawings, in which:

[0018] FIG. 1 illustrates a comparison of curing curves of rubber compounds prepared with unmodified carbon black N234 (A) and sodium sulphide treated modified carbon black N234 (B), in accordance with the present disclosure; and

[0019] FIG. 2 illustrates a comparison of Tan Delta curves of rubber compounds prepared with unmodified carbon black N234 (A) and sodium sulphide treated modified carbon black N234 (B), in accordance with the present disclosure.

DETAILED DESCRIPTION

[0020] The present disclosure envisages a surface modified carbon black, which when combined with a polymer composition, alters the carbon black-polymer interaction to decrease the hysteresis of the polymer composition by at least 1%. The properties of the carbon black that make it a useful additive/reinforcement in the polymer are established in the carbon black during its manufacturing. The properties like particle size, shape and degree of aggregation are controlled by regulating the operating parameters during the manufacturing process. It is found that the surface chemistry of the carbon black, formed in the manufacturing process, impacts the performance of the carbon black as reinforcement in a polymer composition. The surface chemistry of the carbon black can be changed by introducing surface modifying compounds onto the carbon black surface, preferably during the manufacturing of the carbon black. A benefit of altering the surface chemistry of the carbon black is to modify the carbon black-polymer interactions when the carbon black is added to a polymer composition, so as to reduce the hysteresis of the polymer-carbon black compound. The carbon black obtained in accordance with the process of the present disclosure is particularly suitable for making rubber compositions with low hysteresis for use in making tires with low heat build-up.

[0021] The process for producing surface modified carbon black comprises the step of treating carbon black with a sulfur-containing compound in an amount in the range of 0.005%-1% of the carbon black to effect formation of surface groups. The surface modified carbon black thus obtained when combined with a polymer composition alters the carbon black-polymer interaction to decrease the hysteresis of the polymer composition by at least 1%, preferably by about 1% to 20%. The sulfur-containing compound is selected from the group consisting of sodium sulfate, sodium sulfide, sodium sulfite, sodium polysulfide, sodium thiosulfate, phenylene disulfide, alkali metal sulfate, alkali metal sulfite, alkali metal sulfide, alkaline earth metal sulfate, alkaline earth metal sulfite, alkaline earth metal sulfide, and mixtures thereof.

[0022] In accordance with the present disclosure the carbon black is treated with a sulphur-containing compound by a technique selected from the group consisting of pouring, spraying, injecting, dispersing and diffusing.

[0023] The sulfur-containing compound is preferably introduced in the carbon black during the manufacturing of the carbon black in the furnace reactor by a method selected from pouring, spraying, injecting, dispersing and diffusing, resulting in the surface modified carbon black whose surface is treated such as to provide beneficial properties of reduced hysteresis in a polymer composition in which the modified carbon black is used as reinforcement. The sulfur-containing compound can be alternatively added by a technique such as spraying on the carbon black surface post-manufacturing.

[0024] In accordance with the one of the embodiments of the present disclosure the sulfur-containing compound is in the form of dispersion. Typically, the dispersion is prepared by mixing the sulfur-containing compound with a solvent, preferably water, for convenient introduction on the carbon black surface. The sulfur-containing compound can be mixed with process water provided to pelletize the carbon black during the manufacturing process.

[0025] The sulfur-containing compound when added in an amount in the range of 0.005%-1% of the carbon black, results in the formation of surface groups on the carbon black, which alter the carbon black-polymer interactions due to formation of bonds between the carbon black particles and polymer molecules, when added to a polymer composition to reduce the hysteresis of the composition. The lower hysteresis manifests itself in the form of lower tan delta of the composition. Tan delta, the ratio of the viscous component to the elastic component of the response to a deformation, is a measure of the hysteresis of the composition. A lower tan delta indicates a composition with lower hysteresis. The results indicating the reduced Tan Delta in surface modified carbon black are illustrated in the FIG. 2.

[0026] The disclosure will now be described with reference to the following non-limiting examples which do not limit the scope and ambit of the disclosure.

EXAMPLES

Example 1

[0027] 500 g of unpelletized carbon black (N234 grade) was taken in a tray and sprayed uniformly with a solution of 2.5 g Na.sub.2S in water (500 mL), with slow exposure of all surfaces of the carbon black to the solution. The carbon black was turned over several times over a period of 2 hours, to promote good coverage. The resultant modified carbon black was heated in an oven under a reducing atmosphere, at 800 C. for 8 hours, with a turnover of 4-5 times every 2 hours. The dried modified carbon black was used to prepare a rubber compound and tested (Labeled: N234-1-LAB). The properties of this compound were compared with those of a rubber compound prepared using unmodified carbon black N234 (Labeled: N234-UNMOD).

Preparation of Rubber Compound

[0028] The composition of the tested rubber compounds are provided herein below.

TABLE-US-00001 Quantity, parts Ingredients per hundred (pph) Natural Rubber (RSS4 Grade) 75 Butadiene Rubber (1220 Grade) 25 Carbon Black (N234 grade) 50 Zinc Oxide 4 Stearic Acid 2 Antioxidant (6PPD) 1.5 Sulfur 1 Accelerator (CBS) 1

[0029] The ingredients were mixed on a 2-roll mill at a friction ratio of 1:1.4 for a duration of about 24 minutes. The rollers were maintained at a temperature of 70 C.

Testing of Rubber Properties:

[0030] The properties of the prepared rubber compounds were tested. A summary of the test results is given in Table 1.

TABLE-US-00002 TABLE 1 Comparison of properties of rubber compounds using unmodified carbon black N234, and sodium sulfide treated modified carbon black N234, in lab-scale production Maximum Tan % Delta Value Reduction in Loading of (from Rubber Tan Delta vs. Sample Name Na.sub.2S, ppm Process Analyzer) baseline N234-UNMOD 0 0.218 0 (Baseline) N234-1-LAB 5000 0.211 3.21

Example 2

[0031] 100 ppm of sodium sulfide (Na.sub.2S) per unit mass of carbon black, was added to the manufacturing process in the pelletization step, by adding a 2% solution of Na.sub.2S in water (previously prepared) at an appropriate flow-rate into the pelletizer. The treated carbon black was then dried as per the usual industrial process, in a rotary drier. The samples of the treated, pelleted, dried carbon black were collected and compounded with rubber for testing (Labeled: N234-2-IND).

Preparation of Rubber Compound

[0032] The composition of the tested rubber compounds are provided herein below.

TABLE-US-00003 Quantity, parts Ingredients per hundred (pph) Natural Rubber (RSS4 Grade) 75 Butadiene Rubber (1220 Grade) 25 Carbon Black (N234 grade) 50 Zinc Oxide 4 Stearic Acid 2 Antioxidant (6PPD) 1.5 Sulfur 1 Accelerator (CBS) 1

[0033] The ingredients were mixed on a 2-roll mill at a friction ratio of 1:1.4 for a duration of about 24 minutes. The rollers were maintained at a temperature of 70 C.

Testing of Rubber Properties

[0034] The properties of the prepared rubber compounds were tested. A summary of the test results is given in Table 2.

TABLE-US-00004 TABLE 2 Comparison of properties of rubber compounds using unmodified N234, and sodium sulfide treated modified carbon black N234, in industrial process Loading Maximum Tan Reduction in of Delta Value Tan Delta Na2S, (from Rubber vs. baseline, Sample Name ppm Process Analyzer) % N234-UNMOD 0 0.196 0 (Baseline) N234-2-IND 100 0.189 3.57

[0035] From the Examples 1 & 2 it is clearly demonstrated that a significant reduction in tan delta is achieved by both the lab treatment and the industrial treatment. However, the industrial treatment of the carbon black, during its manufacturing, with very small amounts of sodium sulfide, is more effective in reducing the tan delta of the rubber compound.

[0036] The curing curves of the rubber, compounded with the unmodified carbon black N234, and sodium sulfide treated modified carbon black N234 are shown in FIG. 1 of the accompanying drawings. The hysteresis in the rubber compounds prepared using the carbon black is estimated by measuring the curing tan delta of the compound, and is shown in FIG. 2 of the accompanying drawings.

[0037] The curing curves A and B illustrated in the FIG. 1 clearly show that the rubber compound containing the sodium sulfide treated modified carbon black N234 of the present disclosure cures more easily, likely because of the greater interactions between the rubber polymer and the surface groups on the treated carbon black as compared to the rubber compound with the unmodified carbon black. Likewise, the tan delta curves A and B illustrated in the FIG. 2 show that the rubber compound prepared with the sodium sulfide treated modified carbon black N234 of the present disclosure exhibits a lower tan delta, and therefore a lower hysteresis, than the rubber compound prepared with the unmodified carbon black.

Technical Advantages

[0038] The process as described in the present disclosure has several technical advantages including but not limited to the realization of: the disclosure provides a simple and economic process for producing a surface modified carbon black, in which carbon black is treated with a sulfur compound in an amount in the range of 0.005%-1% of the carbon black to effect in-situ formation of surface groups to produce the surface modified carbon black which when combined with a polymer composition alter the carbon black-polymer interaction to decrease the hysteresis of the polymer composition by at least 1%, preferably by about 1% to 20%, the surface modified carbon black is particularly suitable for making high performance tires with reduced hysteresis and low heat build-up.

[0039] Throughout this specification the word comprise, or variations such as comprises or comprising, will be understood to imply the inclusion of a stated element, integer or step, or group of elements, integers or steps, but not the exclusion of any other element, integer or step, or group of elements, integers or steps.

[0040] The use of the expression at least or at least one suggests the use of one or more elements or ingredients or quantities, as the use may be in the embodiment of the invention to achieve one or more of the desired objects or result's.

[0041] Any discussion of documents, acts, materials, devices, articles or the like that has been included in this specification is solely for the purpose of providing a context for the invention. It is not to be taken as an admission that any or all of these matters form part of the prior art base or were common general knowledge in the field relevant to the invention as it existed anywhere before the priority date of this application.

[0042] The numerical values mentioned for the various physical parameters, dimensions or quantities are only approximations and it is envisaged that the values higher/lower than the numerical values assigned to the parameters, dimensions or quantities fall within the scope of the invention, unless there is, a statement in the specification specific to the contrary.

[0043] In view of the wide variety of embodiments to which the principles of the present invention can be applied, it should be understood that the illustrated embodiments are exemplary only. While considerable emphasis has been placed herein on the particular features of this invention, it will be appreciated that various modifications can be made, and that many changes can be made in the preferred embodiments without departing from the principle of the invention. These and other modifications in the nature of the invention or the preferred embodiments will be apparent to those skilled in the art from the disclosure herein, whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the invention and not as a limitation.